CN102850804B - Transparent two-component organic silicon pouring sealant for LED and preparation method thereof - Google Patents
Transparent two-component organic silicon pouring sealant for LED and preparation method thereof Download PDFInfo
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- CN102850804B CN102850804B CN201210300362.3A CN201210300362A CN102850804B CN 102850804 B CN102850804 B CN 102850804B CN 201210300362 A CN201210300362 A CN 201210300362A CN 102850804 B CN102850804 B CN 102850804B
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Abstract
The invention discloses a transparent two-component organic silicon pouring sealant for LED and a preparation method thereof. The pouring sealant comprises a component A and a component B mixed according to a mass ratio of 1:1. The component A comprises vinyl silicone oil, hydrogen-containing silicone oil and methyl vinyl MQ silicone resin in a mass ratio of 100:5-20:20-50; and the B component comprises vinyl silicone oil and a platinum catalyst in a mass ratio of 100:0.01-1.
Description
Technical field
The present invention relates to joint sealant Material Field, particularly relate to LED clear two-component organic silicon potting adhesive that a kind of transparency is strong, mechanical property good and humidity resistance is good and preparation method thereof.
Background technology
At present, the epoxide resin material of LED joint sealant many employings low cost, but the high thermal resistance of epoxy resin, wet fastness are poor.High thermal resistance difference easily damages element, and shorten element work-ing life, wet fastness difference then can cause aqueous vapor easily to enter element internal, easily causes the problems such as short circuit.Along with the continuing to bring out of illumination level LED component of flourish, high-power, high brightness, the long life requirement of LED illumination industry, need a kind of high performance packaged material to meet the requirement of LED.
And existing joint sealant glue sample embrittlement, frangibility, tensile property and flexility all also do not reach the requirement of LED, and use properties has much room for improvement.
Therefore, prior art has yet to be improved and developed.
Summary of the invention
In view of above-mentioned the deficiencies in the prior art, the object of the present invention is to provide a kind of LED clear two-component organic silicon potting adhesive and preparation method thereof, be intended to solve the problem that existing LED encapsulation material high thermal resistance is poor, wet fastness is poor, glue sample embrittlement, flexility and tensile property are not good.
Technical scheme of the present invention is as follows:
The two component transparent organic silicon joint sealant of a kind of LED, wherein, it comprises is component A and the B component of 1:1 mixing in mass ratio;
Described component A comprises:
Vinyl silicone oil;
Containing hydrogen silicone oil;
Methyl vinyl MQ silicon resin;
Described B component comprises:
Vinyl silicone oil;
Platinum catalyst;
Wherein, the mass ratio of the vinyl silicone oil in described component A, containing hydrogen silicone oil and methyl vinyl MQ silicon resin is 100:5 ~ 20:20 ~ 50, and the vinyl silicone oil in described B component and the mass ratio of platinum catalyst are 100:0.01 ~ 1.
The two component transparent organic silicon joint sealant of described LED, wherein, the structure of described vinyl silicone oil is the linear methyl vinyl silicone oil containing two vinyl-functional end groups in each polysiloxane molecule.
The two component transparent organic silicon joint sealant of described LED, wherein, the structure of described containing hydrogen silicone oil is directly be connected with chemical bond with Siliciumatom containing at least two hydrogen atoms in each polysiloxane molecule.
The two component transparent organic silicon joint sealant of described LED, wherein, the hydrogen mass content of described containing hydrogen silicone oil is 0.3 ~ 1.0%.
The two component transparent organic silicon joint sealant of described LED, wherein, the M in described methyl vinyl MQ silicon resin is that single functionality siloxanes closes chain link (CH3)
3siO
1/2(CH
2=CH) (CH
3)
2siO
1/2.
The two component transparent organic silicon joint sealant of described LED, wherein, the Q in described methyl vinyl MQ silicon resin is four functionality siloxane polycondensation chain link SiO
4/2.
The two component transparent organic silicon joint sealant of described LED, wherein, the molecular formula of described methyl vinyl MQ silicon resin is [(CH3)
3siO
1/2]
a[(CH
2=CH) (CH
3)
2siO
1/2]
b[SiO
4/2]
c, wherein, the mol ratio of (a+b)/c is 0.6 ~ 1.2.
The two component transparent organic silicon joint sealant of described LED, wherein, the massfraction of the vinyl in described methyl vinyl MQ silicon resin is 0.1 ~ 10%.
A LED preparation method for two component transparent organic silicon joint sealant, wherein, comprises step:
A, vinyl silicone oil, methyl vinyl MQ silicon resin and containing hydrogen silicone oil are carried out blended for 100:5 ~ 20:20 ~ 50 in mass ratio, heat temperature raising, process 1.5 ~ 2.5 hours under vacuum condition, obtain component A;
B, vinyl silicone oil and platinum catalyst to be mixed for 100:0.01 ~ 1 in mass ratio, are warming up to 100 DEG C, process 1.5 ~ 2.5 hours under vacuum condition B component;
C, by described component A with B component in mass ratio for 1:1 mixes, vacuum defoamation, solidification obtains the two component transparent organic silicon joint sealant of LED at ambient temperature.
Described preparation method, wherein, described component A and B component are all process 2 hours under vacuum to obtain.
Beneficial effect: LED clear two-component organic silicon potting adhesive of the present invention and preparation method thereof, by the vinyl on vinyl silicone oil under the effect of platinum catalyst with the si-h bond generation addition reaction in containing hydrogen silicone oil, generation-CH
2-CH
2-Si-cross-link bond, because reaction discharges without small molecules, so ungauged regions after solidification, it is excellent Embedding Material, prepared joint sealant has good dielectric properties, wider use temperature scope and excellent damping property, joint sealant high thermal resistance of the present invention, wet fastness, tensile property and snappiness significantly improve, and do not affect its transparency.
Embodiment
The invention provides a kind of LED clear two-component organic silicon potting adhesive and preparation method thereof, for making object of the present invention, technical scheme and effect clearly, clearly, the present invention is described in more detail below.Should be appreciated that specific embodiment described herein only in order to explain the present invention, be not intended to limit the present invention.
The two component transparent organic silicon joint sealant of LED provided by the invention, it comprises is component A and the B component of 1:1 mixing in mass ratio;
Described component A comprises:
Vinyl silicone oil;
Containing hydrogen silicone oil;
Methyl vinyl MQ silicon resin;
Described B component comprises:
Vinyl silicone oil;
Platinum catalyst;
Wherein, the mass ratio of the vinyl silicone oil in described component A, containing hydrogen silicone oil and methyl vinyl MQ silicon resin is 100:5 ~ 20:20 ~ 50, and the vinyl silicone oil in described B component and the mass ratio of platinum catalyst are 100:0.01 ~ 1.
Described vinyl silicone oil is the low molecular weight polysiloxane with vinyl on part Siliciumatom, vinyl silicone oil is the main raw material of organic silicon potting adhesive of the present invention, specifically can adopt that the vinyl silicone oil of several different viscosity is composite reaches required viscosity, the viscosity of vinyl silicone oil of the present invention is generally 300 ~ 5000 centipoises (least unit of kinetic viscosity, 1 centipoise equals 0.01 pool).The structure of the vinyl silicone oil adopted in the present invention is the linear methyl vinyl silicone oil containing two vinyl-functional end groups in each polysiloxane molecule, wherein, vinyl molar mass is 0.05 ~ 0.5%, adopts the organic silicon potting adhesive obtained by vinyl silicone oil of said structure to have good elongation, humidity resistance and insulativity.
Described containing hydrogen silicone oil is under metal solvent effect, can be cross-linked at proper temperature, thus improve snappiness and the tensile property of organic silicon potting adhesive, containing hydrogen silicone oil preferred structure of the present invention is containing the containing hydrogen silicone oil that at least two hydrogen atoms are directly connected with chemical bond with Siliciumatom in each polysiloxane molecule, further, the hydrogen mass content of described containing hydrogen silicone oil is 0.3 ~ 1.0%, adopts the organic silicon potting adhesive obtained by containing hydrogen silicone oil of said structure to prove that snappiness is all relative with tensile property better through test.
Described methyl vinyl MQ silicon resin is the organic resin be made up of four functionality siloxane polycondensation chain links (Q) and single functionality siloxane unit (M), and its Main Function is intended for strengthening agent.The when structures shape character of resin of the amount of M chain link and Q chain link in the molecular structure of described methyl vinyl MQ silicon resin.M chain link in the present invention is preferably single functionality siloxanes and closes chain link (CH3)
3siO
1/2(CH
2=CH) (CH
3)
2siO
1/2, and Q chain link is preferably four functionality siloxane polycondensation chain link SiO
4/2.Further, the structure of described methyl vinyl MQ silicon resin is [(CH3)
3siO
1/2]
a[(CH
2=CH) (CH
3)
2siO
1/2]
b[SiO
4/2]
c, wherein, the mol ratio of (a+b)/c is 0.6 ~ 1.2.Adopt the methyl vinyl MQ silicon resin of said structure that the tensile strength of last obtained organic silicon potting adhesive glue sample and snappiness can be made greatly to strengthen, and do not affect the transparency, thus improved the bad problem of the sample embrittlement that removes photoresist, frangibility, use properties.
Preferably, the massfraction of the vinyl in described methyl vinyl MQ silicon resin is 0.1 ~ 1.0%, to improve tensile strength and the snappiness of organic silicon potting adhesive further.
Described platinum catalyst, mainly with the platinum catalyst of Platinic chloride precious metal for main raw material activeconstituents, adopts wire netting, platinum black or platinum is loaded on the carriers such as aluminum oxide.The catalytic efficiency of platinum catalyst is high, and anti-yellowing property is good, high reactivity, has higher stability in use.
The present invention also provides a kind of LED preparation method of two component transparent organic silicon joint sealant, and it comprises step:
A, vinyl silicone oil, methyl vinyl MQ silicon resin and containing hydrogen silicone oil are carried out blended for 100:5 ~ 20:20 ~ 50 in mass ratio, heat temperature raising, process 1.5 ~ 2.5 hours under vacuum condition, obtain component A;
B, vinyl silicone oil and platinum catalyst to be mixed for 100:0.01 ~ 1 in mass ratio, are warming up to 100 DEG C, process 1.5 ~ 2.5 hours under vacuum condition B component;
C, by described component A with B component in mass ratio for 1:1 mixes, vacuum defoamation, solidification obtains the two component transparent organic silicon joint sealant of LED at ambient temperature.
Further, described heat temperature raising is for being heated to 100 DEG C, and described vacuum condition is-0.06MPa, and even more preferably respectively under vacuum process within 2 hours, obtain component A and B component, now sufficient reacting, component A and the B component of better performances can be obtained.
Before step c, component A and B component prepared and distinguish packaging and storing, be that 1:1 mixes according to mass ratio in use, vacuum defoamation about 5 minutes, encapsulates LED component, and then leaves standstill 2 ~ 4h under room temperature condition and can solidify completely.
The two component transparent organic silicon joint sealant of LED that the present invention adopts aforesaid method to obtain has good thermotolerance, wet fastness, intensity is high, packaging effect is good feature, can available protecting LED component, and manufacture craft is simple.In addition, LED prepared by the present invention, with two component transparent organic silicon joint sealant transparency is good, snappiness is good, color inhibition, has esy to use, safe and reliable, environmentally safe, stable performance, the feature such as can not to ftracture at low temperatures.In the encapsulation of LED, not only play certain mechanical support, the effect of sealed environment, good printing opacity, protection against the tide, dust-proof, protection against corrosion and shockproof effect can also be played.
Below in conjunction with embodiment, the present invention will be described, vinyl silicone oil in following embodiment is and adopts structure to be the linear methyl vinyl silicone oil each polysiloxane molecule containing two vinyl-functional end groups, and vinyl molar mass mark is 0.05 ~ 0.5%; Methyl vinyl MQ silicon resin is [(CH3)
3siO
1/2]
a[(CH
2=CH) (CH
3)
2siO
1/2]
b[SiO
4/2]
c, wherein, the mol ratio of (a+b)/c is 0.6 ~ 1.2, and the massfraction of vinyl is 0.1 ~ 10%; Containing hydrogen silicone oil structure is directly be connected with chemical bond with Siliciumatom containing at least two hydrogen atoms in polysiloxane per molecule, and hydrogen mass content is 0.3 ~ 1.0%.
Embodiment 1
Get the vinyl silicone oil 100g that viscosity is 400 centipoises, methyl vinyl MQ silicon resin 5g, viscosity is the containing hydrogen silicone oil 20g of 200 centipoises, mixes in kneader, is warming up to 100 DEG C, and vacuum-0.06MPa processes 1.5 hours, obtains component A.Get the vinyl silicone oil 100g that viscosity is 400 centipoises, platinum catalyst 0.01g, mixes in planet stirring tank, is warming up to 100 DEG C, and vacuum-0.06MPa processes 1.5 hours, composition B component.Before use, A, B component are prepared and distinguish packaging and storing, according to weight ratio 1:1 mixing during use, vacuum defoamation 5 minutes, encapsulates LED lamp, and then at room temperature leaving standstill 2-4h can solidify completely.
Embodiment 2
Get the vinyl silicone oil 100g that viscosity is 1000 centipoises, methyl vinyl MQ silicon resin 10g, viscosity is the containing hydrogen silicone oil 30g of 100 centipoises, mixes in kneader, is warming up to 100 DEG C, and vacuum-0.06MPa processes 2 hours, obtains component A.Get the vinyl silicone oil 100g that viscosity is 1000 centipoises, platinum catalyst 0.1g, mixes in planet stirring tank, is warming up to 100 DEG C, and vacuum-0.06MPa processes 2 hours, composition B component.Before use, A, B component are prepared and distinguish packaging and storing, according to weight ratio 1:1 mixing during use, vacuum defoamation 5 minutes, encapsulates LED lamp, and then at room temperature leaving standstill 2-4h can solidify completely.
Embodiment 3
Get the vinyl silicone oil 100g that viscosity is 4000 centipoises, methyl vinyl MQ silicon resin 20g, viscosity is the containing hydrogen silicone oil 40g of 50 centipoises, mixes in kneader, is warming up to 100 DEG C, and vacuum-0.06MPa processes 2.5 hours, obtains component A.Get the vinyl silicone oil 100g that viscosity is 4000 centipoises, platinum catalyst 0.5g, mixes in planet stirring tank, is warming up to 100 DEG C, and vacuum-0.06MPa processes 2.5 hours, composition B component.Before use, A, B component are prepared and distinguish packaging and storing, according to weight ratio 1:1 mixing during use, vacuum defoamation 5 minutes, encapsulates LED lamp, and then at room temperature leaving standstill 2-4h can solidify completely.
Contrast sample
Get the vinyl silicone oil 100g that viscosity is 4000 centipoises, viscosity is the containing hydrogen silicone oil 40g of 50 centipoises, mixes in kneader, is warming up to 100 DEG C, and vacuum-0.06MPa processes 2 hours, obtains component A.Get the vinyl silicone oil 100g that viscosity is 4000 centipoises, platinum catalyst 0.5g, mixes in planet stirring tank, is warming up to 100 DEG C, and vacuum-0.06MPa processes 2 hours, composition B component.Before use, A, B component are prepared and distinguish packaging and storing, according to weight ratio 1:1 mixing during use, vacuum defoamation 5 minutes, encapsulates LED lamp, and then at room temperature leaving standstill 2-4h can solidify completely.
Table one performance test table
| Test event | Unit | Testing method | Instrument | Example 1 product | Example 2 product | Example 3 product | Contrast sample |
| Outward appearance | — | Range estimation | Range estimation | Water white transparency | Water white transparency | Water white transparency | Water white transparency |
| Hardness | Shore A | GB/T 531-1999 | Sclerometer | 30 | 22 | 18 | 13 |
| Proportion | g/cm 3 | GB/T 533-2008 | Densometer | 0.95 | 0.98 | 1.00 | 0.92 |
| Surface drying time | min | ASTM 0242 | － | 23 | 17 | 10 | 10 |
| Tensile strength | MPa | GB/T 528-2009 | Puller system | 1.31 | 1.16 | 0.95 | 0.43 |
| Elongation at break | % | GB/T 528-2009 | Puller system | 117 | 152 | 183 | 78 |
| Humidity resistance | — | GB2423.34-1986 | Climatic chamber | Well | Well | Well | Generally |
| Specific inductivity | (1MHz) | GB/T1693-2007 | HF Q meter | 2.8 | 2.7 | 2.7 | 2.7 |
| Dielectric loss tangent value | (1MHz) | GB/T1693-2007 | HF Q meter | 0.001 | 0.001 | 0.001 | 0.001 |
From table one: adopt the LED product that the present invention makes, not only transmittance, good fluidity, and there is the advantages such as good elongation, humidity resistance, insulativity, have good dielectric properties in addition, various aspects of performance is obviously better than epoxy resin material.And after adding methyl vinyl MQ silicon resin, its mechanical property such as tensile strength and elongation at break significantly improve, and do not affect its transparency.
In sum, the present invention is alkene addition reaction of hydrogen by the curing mechanism of two-component addition type room temperature vulcanized silicone rubber, vinyl on vinyl silicone oil under the effect of platinum catalyst with the si-h bond generation addition reaction in containing hydrogen silicone oil, generation-CH2-CH2-Si-cross-link bond, because reaction discharges without small molecules, so ungauged regions after solidification, it is excellent Embedding Material.It has good dielectric properties, and wider use temperature scope and excellent damping property, use more and more general in LED embedding industry.Do not add the transparent of reinforced filling and add plastic glue sample embrittlement, frangibility, use properties is bad.
Should be understood that, application of the present invention is not limited to above-mentioned citing, for those of ordinary skills, can be improved according to the above description or convert, and all these improve and convert the protection domain that all should belong to claims of the present invention.
Claims (2)
1. the two component transparent organic silicon joint sealant of LED, is characterized in that, it comprises is component A and the B component of 1:1 mixing in mass ratio;
Described component A comprises:
Viscosity is the vinyl silicone oil of 400 centipoises, 100g;
Viscosity is the containing hydrogen silicone oil of 200 centipoises, 20g;
Methyl vinyl MQ silicon resin, 5g;
Described B component comprises:
Viscosity is the vinyl silicone oil of 400 centipoises, 100g;
Platinum catalyst, 0.01g;
The structure of described vinyl silicone oil is the linear methyl vinyl silicone oil containing two vinyl-functional end groups in each polysiloxane molecule, and described vinyl molar mass is 0.05 ~ 0.5%;
The structure of described containing hydrogen silicone oil is directly be connected with chemical bond with Siliciumatom containing at least two hydrogen atoms in each polysiloxane molecule, and the hydrogen mass content of described containing hydrogen silicone oil is 0.3 ~ 1.0%;
M in described methyl vinyl MQ silicon resin is that single functionality siloxanes closes chain link (CH
3)
3siO
1/2(CH
2=CH) (CH
3)
2siO
1/2;
Q in described methyl vinyl MQ silicon resin is four functionality siloxane polycondensation chain link SiO
4/2; The molecular formula of described methyl vinyl MQ silicon resin is [(CH
3)
3siO
1/2]
a[(CH
2=CH) (CH
3)
2siO
1/2]
b[SiO
4/2]
c, wherein, the mol ratio of (a+b)/c is 0.6 ~ 1.2.
2. a LED as claimed in claim 1 preparation method for two component transparent organic silicon joint sealant, is characterized in that, comprise step:
A, vinyl silicone oil, methyl vinyl MQ silicon resin and containing hydrogen silicone oil are carried out in mass ratio in kneader blended, be heated to 100 DEG C, process 1.5 hours under vacuum-0.06MPa condition, obtain component A;
B, vinyl silicone oil and platinum catalyst to be mixed in mass ratio in planet stirring tank, are warming up to 100 DEG C, process 1.5 hours under vacuum-0.06MPa condition B component;
C, by described component A with B component in mass ratio for 1:1 mixes, vacuum defoamation 5 minutes, leaves standstill 2 ~ 4h solidification at ambient temperature and obtains the two component transparent organic silicon joint sealant of LED.
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| CN103131190B (en) * | 2013-02-05 | 2015-07-01 | 广州市爱易迪新材料科技有限公司 | Double-component self-molding lens silica gel for light-emitting diode (LED) package and package process of double-component self-molding lens silica gel |
| JP6497072B2 (en) * | 2013-11-07 | 2019-04-10 | 東レ株式会社 | Laminated body and method of manufacturing light emitting device using the same |
| CN103589387B (en) * | 2013-11-20 | 2015-08-05 | 广州集泰化工股份有限公司 | LED high strength bonding self-vulcanizing organic silicon potting adhesive and preparation method thereof |
| CN103865270B (en) * | 2014-03-14 | 2017-05-10 | 绵阳惠利电子材料有限公司 | Addition silicone rubber compound for protecting diode chip |
| CN104497580B (en) * | 2014-12-04 | 2018-03-16 | 江苏天辰新材料股份有限公司 | A kind of dual composition addition type high fire-retardance Silica hydrogel of low compressive deformation and preparation method thereof |
| CN105860083B (en) * | 2016-04-14 | 2018-12-07 | 顺德职业技术学院 | The preparation method of the organosilicon sealing of the silicone resin containing modified vinyl |
| CN106098915A (en) * | 2016-06-21 | 2016-11-09 | 阜阳市光普照明科技有限公司 | A kind of nano-perovskite modified silica-gel being applied to LED plant growth lamp chip package |
| CN106497470A (en) * | 2016-11-02 | 2017-03-15 | 常州市鼎升环保科技有限公司 | A kind of preparation method of high viscosity aging resistance casting glue |
| CN108424652B (en) * | 2018-04-16 | 2020-10-02 | 吉林大学 | Addition type silica gel and preparation method and application thereof |
| CN109320969A (en) * | 2018-09-28 | 2019-02-12 | 唐山市第中学 | Anti-blue light film is at film liquid and preparation method thereof and anti-blue light film |
| CN111207173B (en) * | 2020-01-09 | 2021-11-16 | 苏州赛伍应用技术股份有限公司 | Buffering silica gel sheet used between electric cores of power battery pack, preparation method of buffering silica gel sheet and power battery pack comprising buffering silica gel sheet |
| CN114958288B (en) * | 2021-02-27 | 2023-12-08 | 华为技术有限公司 | Organic silicon conductive adhesive, crystal oscillator and electronic equipment |
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| CN102382618A (en) * | 2011-08-25 | 2012-03-21 | 江苏创景科技有限公司 | Two-component high strength transparent room temperature solidified organosilicon casting glue |
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Address after: 518057, Qiong Yu Road, Nanshan District science and Technology Park, Shenzhen, Guangdong, 6 Patentee after: Shenzhen Tianding new materials Co. Ltd. Address before: 518057, Qiong Yu Road, Nanshan District science and Technology Park, Shenzhen, Guangdong, 6 Patentee before: Shenzhen Tianding Fine Chemical Co., Ltd. |